CN103951429B - A kind of low-temperature sintering low-loss microwave dielectric ceramic materials - Google Patents
A kind of low-temperature sintering low-loss microwave dielectric ceramic materials Download PDFInfo
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- CN103951429B CN103951429B CN201410166373.6A CN201410166373A CN103951429B CN 103951429 B CN103951429 B CN 103951429B CN 201410166373 A CN201410166373 A CN 201410166373A CN 103951429 B CN103951429 B CN 103951429B
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- temperature sintering
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Abstract
The invention discloses a kind of low-temperature sintering low-loss microwave dielectric ceramic materials, its chemical formula is Ni
0.04zn
0.96tiNb
2o
8+ (1 ~ 4) wt%B
2o
3, adopt chemical feedstocks ZnO, NiO, Nb
2o
5and TiO
2, in 900 ~ 940 DEG C of sintering.The present invention is at ZnTiNb
2o
8on the basis of system's pottery, use B
2o
3as sintering aid, provide a kind of low sintering ceramics as low-loss microwave medium material and preparation method thereof, and maintain dielectric properties relatively preferably simultaneously.Its sintering temperature is 900 ~ 940 DEG C, and specific inductivity is 30 ~ 36, and quality factor are 32,100 ~ 39,500GHz, and temperature coefficient of resonance frequency is-32 ~-39 × 10
-6/ DEG C.In addition, preparation technology of the present invention is simple, and process is pollution-free, has broad application prospects.
Description
Technical field
The invention belongs to a kind of take composition as the ceramic composition of feature, particularly a kind of low-temperature sintering low-loss microwave dielectric ceramic materials.
Background technology
In recent years, along with the fast development of radar and the communication technology, the requirement of the miniaturization of all kinds of microwave mobile communication terminating unit, lightweight, multifunction and cost degradation is improved constantly.Can effectively reduce device volume with the multi-layer structure design based on LTCC (low-temperature co-firedceramic, LTCC) technology, be realize components and parts to miniaturization, integrated and modular important channel.The preparation of multiplayer microwave components and parts, microwave-medium ceramics and high conductivity electrode is needed to burn altogether, therefore, low-temperature co-fired microwave components and parts are had higher requirement to microwave-medium ceramics, in order to burn altogether in an atmosphere with the metal electrode of the high conductivity such as Ag (fusing point is 961 DEG C), the sintering temperature of microwave-medium ceramics will drop to less than 950 DEG C.Interpolation low melting point oxide or glass sintering auxiliary agent are a kind of modal methods reducing sintering temperature to reduce the sintering temperature of microwave dielectric material.
ZnTiNb
2o
8system's pottery has relatively low sintering temperature (1080 DEG C), is expected to realize low-temperature sintering when adulterating a small amount of sintering aid, meanwhile keeps dielectric properties relatively preferably.
Summary of the invention
Object of the present invention, at ZnTiNb
2o
8on the basis of system's pottery, use B
2o
3as sintering aid, provide a kind of low sintering ceramics as low-loss microwave medium material and preparation method thereof, and keep dielectric properties relatively preferably simultaneously.
The present invention is achieved by following technical solution.
A kind of low-temperature sintering low-loss microwave dielectric ceramic materials, chemical formula Ni
0.04zn
0.96tiNb
2o
8+ (1 ~ 4) wt%B
2o
3;
The preparation method of this low-temperature sintering low-loss microwave-medium ceramics material, has following steps:
(1) by chemical feedstocks ZnO, NiO, Nb
2o
5and TiO
2press Ni respectively
0.04zn
0.96tiNb
2o
8stoichiometric ratio weigh batching.
(2) chemical feedstocks mixing step (1) configured, puts into ball grinder, then adds zirconia ball and deionized water, ball milling 4 ~ 6 hours, then dried in infrared drying oven by the raw material after ball milling, sieve;
(3) powder step (2) mixed, in 850 DEG C of calcinings, is incubated 3 hours, synthesis presoma;
(4) in the presoma synthesized in step (3) additional mass percent be 0.70 ~ 1.05% polyvinyl alcohol and mass percent be the B of (1 ~ 4) %
2o
3, put into ball grinder, then add zirconia ball and deionized water, ball milling 8 ~ 12 hours, sieves after oven dry, then is base substrate with powder compressing machine pressure forming;
(5) by base substrate in 900 ~ 940 DEG C of sintering, be incubated 3 ~ 6 hours, make low-temperature sintering low-loss microwave dielectric ceramic materials;
(6) microwave dielectric property of network analyzer test for low temperature sintering ceramics as low-loss microwave medium material is adopted.
The purity of the chemical feedstocks of described step (1) is greater than 99.9%.
The powder compressing machine of described step (4) is with the pressure forming of 3 ~ 7MPa, and base substrate is the right cylinder of Φ 10mm × 5mm;
The preferred sintering temperature of described step (5) is 940 DEG C.
Ni of the present invention
0.04zn
0.96tiNb
2o
8+ (1 ~ 4) wt%B
2o
3low-temperature sintering low-loss microwave dielectric ceramic materials, its sintering temperature is 900 ~ 940 DEG C, and specific inductivity is 30 ~ 36, and quality factor are 32,100 ~ 39,500GHz, and temperature coefficient of resonance frequency is-32 ~-39 × 10
-6/ DEG C.In addition, preparation technology of the present invention is simple, and process is pollution-free, has broad application prospects.
Embodiment
The present invention adopts purity to be greater than chemical feedstocks ZnO, NiO, Nb of 99.9%
2o
5, TiO
2and B
2o
3preparation Ni
0.04zn
0.96tiNb
2o
8+ (1 ~ 4) wt%B
2o
3microwave-medium ceramics, specific embodiment is as follows:
Embodiment 1
1) by ZnO, NiO, Nb
2o
5, TiO
2difference 0.96:0.04:1:1 weigh batching in molar ratio;
2) add in nylon tank after the raw material configured being mixed, ball milling 6 hours; Again the raw material after ball milling is placed in infrared drying oven to dry, sieves;
3) by the raw material after sieving, in 850 DEG C of calcinings, 3 hours are incubated, synthesis precursor;
4) in the precursor of synthesis, additional mass percent is 1.05% polyvinyl alcohol and mass percent is the B of 1%
2o
3, put into ball grinder, add zirconia ball and deionized water ball milling 10 hours, then dry, sieve; Be pressed into the cylinder shape base substrate of Φ 10mm × 5mm again with the pressure of 8MPa with powder compressing machine;
5) by cylinder shape base substrate in 940 DEG C of sintering, be incubated 5 hours;
6) microwave dielectric property of network analyzer testing example 1 is adopted; Obtain its performance as follows:
Specific inductivity is: 35.97
Quality factor are: 39413GHz
Temperature coefficient of resonance frequency is :-32 × 10
-6
The preparation process of embodiment 2 ~ 5 is substantially the same manner as Example 1, and difference is sintering temperature and B
2o
3addition different; The concrete sintering temperature of embodiment 2 ~ 5 and B
2o
3addition and relevant dielectric properties refer to table 1.
Table 1
Claims (4)
1. a low-temperature sintering low-loss microwave dielectric ceramic materials, chemical formula Ni
0.04zn
0.96tiNb
2o
8+ (1 ~ 4) wt%B
2o
3;
The preparation method of this low-temperature sintering low-loss microwave-medium ceramics material, has following steps:
(1) by chemical feedstocks ZnO, NiO, Nb
2o
5and TiO
2press Ni respectively
0.04zn
0.96tiNb
2o
8stoichiometric ratio weigh batching;
(2) chemical feedstocks mixing step (1) configured, puts into ball grinder, then adds zirconia ball and deionized water, ball milling 4 ~ 6 hours, then dried in infrared drying oven by the raw material after ball milling, sieve;
(3) powder step (2) mixed, in 850 DEG C of calcinings, is incubated 3 hours, synthesis presoma;
(4) in the presoma synthesized in step (3) additional mass percent be 0.70 ~ 1.05% polyvinyl alcohol and mass percent be the B of (1 ~ 4) %
2o
3, put into ball grinder, then add zirconia ball and deionized water, ball milling 8 ~ 12 hours, sieves after oven dry, then is base substrate with powder compressing machine pressure forming;
(5) by base substrate in 900 ~ 940 DEG C of sintering, be incubated 3 ~ 6 hours, make low-temperature sintering low-loss microwave dielectric ceramic materials;
(6) microwave dielectric property of network analyzer test for low temperature sintering ceramics as low-loss microwave medium material is adopted.
2. a kind of low-temperature sintering low-loss microwave dielectric ceramic materials according to claim 1, is characterized in that, the purity of the chemical feedstocks of described step (1) is greater than 99.9%.
3. a kind of low-temperature sintering low-loss microwave dielectric ceramic materials according to claim 1, is characterized in that, the powder compressing machine of described step (4) is with the pressure forming of 3 ~ 7MPa, and base substrate is the right cylinder of Φ 10mm × 5mm.
4. a kind of low-temperature sintering low-loss microwave dielectric ceramic materials according to claim 1, is characterized in that, the preferred sintering temperature of described step (5) is 940 DEG C.
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|---|---|---|---|
| CN201410166373.6A CN103951429B (en) | 2014-04-23 | 2014-04-23 | A kind of low-temperature sintering low-loss microwave dielectric ceramic materials |
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|---|---|---|---|
| CN201410166373.6A CN103951429B (en) | 2014-04-23 | 2014-04-23 | A kind of low-temperature sintering low-loss microwave dielectric ceramic materials |
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| Publication Number | Publication Date |
|---|---|
| CN103951429A CN103951429A (en) | 2014-07-30 |
| CN103951429B true CN103951429B (en) | 2015-10-07 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104987071A (en) * | 2015-07-24 | 2015-10-21 | 天津大学 | Low-temperature sintered microwave dielectric ceramic material with middle permittivity |
| CN105236966A (en) * | 2015-08-31 | 2016-01-13 | 天津大学 | Low-temperature-sintered zinc-titanium-niobium-series microwave dielectric ceramic |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617142A (en) * | 2012-04-05 | 2012-08-01 | 天津大学 | Novel medium-temperature-sintering temperature stabilization type microwave dielectric ceramic |
| CN103467093A (en) * | 2013-08-28 | 2013-12-25 | 天津大学 | Nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and preparation method thereof |
-
2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617142A (en) * | 2012-04-05 | 2012-08-01 | 天津大学 | Novel medium-temperature-sintering temperature stabilization type microwave dielectric ceramic |
| CN103467093A (en) * | 2013-08-28 | 2013-12-25 | 天津大学 | Nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| B2O3与CuO掺杂的ZnO-2TiO2-Nb2O5陶瓷与银电极的共烧行为研究;陈秀丽 等;《功能材料》;20101231;224-226 * |
| Phase composition and microwave dielectric properties of (Zn, Ni)TiNb2O8 solid solution;TianKai Chen et al;《J Mater Sci: Mater Electron》;20140330;2494-2500 * |
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